تفاعل #61501

ord-c63079a6f7f1435894ec7d9308a93c8f

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe solvent evaporated
  2. 2
    أخرىThe residue was partitioned between ethyl acetate (100 ml) and water (100 ml)
  3. 3
    درجة الحرارةcooled to 0° C
  4. 4
    أخرىthe layers separated
  5. 5
    استخلاصThe aqueous layer was further extracted with cold ethyl acetate (100 ml)
  6. 6
    غسيلthe combined organic layers washed with brine (100 ml)
  7. 7
    تجفيفdried (Na2SO4)
  8. 8
    أخرىThe solvents were evaporated

الإجراء التجريبي

4-[1,3]Dioxan-2-yl-butyric acid methyl ester (6.8 g, 0.036 mol) was added to a stirred solution of sodium hydroxide (1.87 g, 0.047 mol) in water (30 ml) and methanol (30 ml). The mixture was stirred for 18 h at room temperature and then the solvent evaporated. The residue was partitioned between ethyl acetate (100 ml) and water (100 ml) and cooled to 0° C. The mixture was acidified with hydrochloric acid (1M) to pH 2 and the layers separated. The aqueous layer was further extracted with cold ethyl acetate (100 ml) and the combined organic layers washed with brine (100 ml) and then dried (Na2SO4). The solvents were evaporated and the crude solid (5.56 g) was used in the next step.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07429579B2uspto-grants-2008_09